CN113622187B - Supercritical carbon dioxide after-finishing process of wave-absorbing electromagnetic shielding fabric - Google Patents
Supercritical carbon dioxide after-finishing process of wave-absorbing electromagnetic shielding fabric Download PDFInfo
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- CN113622187B CN113622187B CN202111038033.1A CN202111038033A CN113622187B CN 113622187 B CN113622187 B CN 113622187B CN 202111038033 A CN202111038033 A CN 202111038033A CN 113622187 B CN113622187 B CN 113622187B
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 239000004744 fabric Substances 0.000 title claims abstract description 88
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 61
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 61
- 238000007730 finishing process Methods 0.000 title claims abstract description 22
- 239000002131 composite material Substances 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 31
- 239000011358 absorbing material Substances 0.000 claims description 30
- 239000000835 fiber Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 28
- 239000012530 fluid Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 239000002041 carbon nanotube Substances 0.000 claims description 18
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 18
- 239000011858 nanopowder Substances 0.000 claims description 18
- 229910000859 α-Fe Inorganic materials 0.000 claims description 14
- 229910021389 graphene Inorganic materials 0.000 claims description 12
- 230000009471 action Effects 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000004753 textile Substances 0.000 claims description 6
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 4
- 238000009792 diffusion process Methods 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 238000005411 Van der Waals force Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
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- 230000005855 radiation Effects 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 13
- 238000012360 testing method Methods 0.000 description 9
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 8
- 239000003063 flame retardant Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 4
- 229920000297 Rayon Polymers 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000002310 reflectometry Methods 0.000 description 4
- 239000004760 aramid Substances 0.000 description 3
- 229920003235 aromatic polyamide Polymers 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
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- 238000007781 pre-processing Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 208000003251 Pruritus Diseases 0.000 description 1
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- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007803 itching Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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- 238000007747 plating Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/76—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon oxides or carbonates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/49—Oxides or hydroxides of elements of Groups 8, 9,10 or 18 of the Periodic Table; Ferrates; Cobaltates; Nickelates; Ruthenates; Osmates; Rhodates; Iridates; Palladates; Platinates
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/12—Aldehydes; Ketones
- D06M13/127—Mono-aldehydes, e.g. formaldehyde; Monoketones
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/0083—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive non-fibrous particles embedded in an electrically insulating supporting structure, e.g. powder, flakes, whiskers
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a supercritical carbon dioxide after-finishing process of a wave-absorbing electromagnetic shielding fabric, which is characterized in that the after-finishing process is carried out by supercritical carbon dioxide, and the after-finishing process is free of water participation, so that the technical problem that composite wave-absorbing powder is difficult to uniformly disperse in a water phase can be solved. The wave-absorbing electromagnetic shielding fabric treated by the post-finishing processing mode has the characteristics of thin thickness, light weight, wide frequency band, strong reflection loss capacity and the like, has flame retardance and radiation resistance, can be used for developing various electromagnetic shielding safety protective clothing, and is widely applied to civil and military fields.
Description
Technical Field
The invention relates to the technical field of functional textiles, in particular to a preparation method of an electromagnetic shielding fabric and a supercritical carbon dioxide after-finishing process.
Background
With the development of intelligent communication systems, wireless network devices, electronic detection devices and other technologies, electromagnetic pollution, which is invisible, inapplicable and inaudible, has started to relate to the living surroundings of people, endanger the health of people and is one of the world public hazards. In order to effectively shield electromagnetic wave interference and reduce harm of electromagnetic waves to human beings and the environment, it is important to develop efficient electromagnetic shielding fabrics.
The earliest people develop electromagnetic shielding protective clothing by utilizing mixed woven fabrics of metal wires and clothing fibers, which has a certain shielding effect on electromagnetic radiation, but has harder hand feeling, thicker and heavier hand feeling and poorer wearing performance. On the basis, the metal fiber blended fabric has the advantage that the wearability of the metal fiber blended fabric is greatly improved. However, since a plurality of fibers are difficult to uniformly mix, the shielding performance is not ideal, and there are also phenomena of tip discharge and itching. Then silver plating fabrics and fabrics containing multiple elements or multiple ions are generated, the electromagnetic shielding fabrics mainly reflect electromagnetic waves and bring secondary pollution to the electromagnetic waves, and the shielding materials mainly absorbing the electromagnetic waves can convert the electromagnetic wave energy into other forms of energy so as to achieve the shielding effect. Based on this, development of a wave-absorbing electromagnetic shielding fabric is imperative.
CN109208333a discloses a method for constructing a wave-absorbing electromagnetic shielding composite coated fabric, which is to soak cotton fabric pretreated by alkali liquor in carbon nanotube dispersion liquid for coating treatment, then sequentially soak by pyrrole solution and oxidize and polymerize by oxidant to form a carbon nanotube/polypyrrole coated fabric, and finally sequentially soak by acid and dry in vacuum. The invention prepares the electromagnetic shielding fabric with shielding effectiveness exceeding 20dB in the frequency band of 3.5-6GHz by utilizing a step-by-step assembly technology, and can meet the commercial shielding requirement.
CN107988787a discloses a method for preparing a wave-absorbing electromagnetic shielding fabric, which comprises the following steps: step 1, soaking cotton fabric in alkali liquor, oscillating at constant temperature, washing with water to neutrality, and drying; step 2, preparing a carbon nano tube dispersion liquid, wherein the concentration ratio of the carbon nano tube to the surfactant in the dispersion liquid is 0.05-0.25:1; step 3, soaking the cotton fabric dried in the step 1 in the carbon nano tube dispersion liquid; and 4, taking out the cotton fabric impregnated in the step 3, and drying to obtain the finished product. The finishing process disclosed by the invention is free from participation of water in the whole process and has the characteristic of dynamic circulation, so that the prepared electromagnetic shielding fabric is excellent in shielding and wave absorbing performance.
There are two ways to develop wave-absorbing electromagnetic shielding fabrics. One is to prepare the wave-absorbing fiber by using a magnetic conductive wave-absorbing material with magnetic conductive property, such as ferrite, metal micropowder (including carbonyl metal and magnetic metal micropowder) and the like. In the process of preparing the fiber, the prepared fiber has a wave absorbing function, the addition amount of the wave absorbing material in the polymer matrix cannot be too low, and the addition amount of the wave absorbing material can cause that the prepared fiber performance is difficult to meet the basic requirements of the fiber for spinning. The other electromagnetic shielding fabric development method adopts coating finishing, but the processing procedure is relatively complex, and the treated fabric has hard hand feeling, poor washing resistance and oxidation resistance, high cost and great difficulty in practical production and application.
The supercritical fluid technology is widely used due to the advantages of high efficiency, environment friendliness, high diffusion coefficient, strong dissolution capability and the like. Wherein carbon dioxide can be converted into a supercritical fluid at a lower temperature and pressure, and can dissolve various nonpolar substances.
The invention adopts supercritical CO 2 The fluid technology forms a supercritical fluid dissolved composite wave-absorbing material under certain temperature and pressure, and the supercritical carbon dioxide fluid has extremely strong diffusion performance, so that the shielding material (graphene, carbon nano tube, ferrite and MXene-Ti) 3 C 2 Etc.) are in a dispersed state and are further loaded into the interior of the fiber matrix. The wave-absorbing electromagnetic shielding fabric treated by the post-finishing processing mode has the characteristics of thin thickness, light weight, wide frequency band, strong reflection loss capacity and the like, has flame retardance and radiation resistance, can be used for developing various electromagnetic shielding safety protective clothing, and is widely applied to civil and military fields.
Disclosure of Invention
The embodiment of the invention provides a supercritical carbon dioxide after-treatment process of a wave-absorbing electromagnetic shielding fabric, which aims to solve the defects that the traditional electromagnetic shielding fabric is easy to corrode, oxidize or react with other chemical substances, is difficult to process, has high density and limited physical elasticity, is easy to generate vortex, has secondary pollution and the like.
Specifically, the invention provides a supercritical carbon dioxide after-finishing process of a wave-absorbing electromagnetic shielding fabric, which comprises the following steps:
the finishing method is a supercritical carbon dioxide after-finishing process, the after-finishing process is free of water participation, and the technical problem that composite wave-absorbing powder is difficult to uniformly disperse in a water phase can be solved.
The method comprises the following specific steps:
(1) Pretreatment of fabrics: the fabric pretreatment agent is one or a mixture of ethanol and acetone, and is dried for standby after treatment.
(2) Post-treatment of supercritical carbon dioxide: taking a certain amount of fabric treated in the step (1), placing the fabric in a high-temperature high-pressure reaction kettle, placing a certain amount of mixture of wave-absorbing nano powder and entrainer in a feeding kettle, introducing carbon dioxide fluid in a supercritical state after heating and pressurizing into the feeding kettle at a certain flow rate, mixing and dissolving the carbon dioxide fluid, the wave-absorbing nano powder and the entrainer to form a finishing agent, and making the formed finishing agent flow back and forth between the feeding kettle and the reaction kettle along with the supercritical carbon dioxide fluid under the action of a circulating device; under the conditions of certain process temperature and pressure, the composite wave-absorbing material dissolved in the supercritical carbon dioxide fluid is fully contacted with the fabric and then dispersed into the fiber to realize after-finishing;
(3) Post-treatment: after a period of time, the reaction temperature and pressure are reduced to enable the unused wave-absorbing powder and CO 2 Separating in a separating kettle, and recycling the unfinished wave-absorbing material, and simultaneously, gaseous CO 2 The reflux collection can also achieve the recycling; thus, the complete post-finishing process is completed.
In some preferred embodiments, the fabric is blended from two or more fibers of inherently flame retardant fibers such as meta-aramid, flame retardant viscose, flame retardant polyester, and the like.
In some preferred embodiments, the fabric pretreatment temperature is 40-60 ℃, the treatment time is 40-60 min, and the drying temperature is 60-80 ℃.
In some preferred embodiments, the wave-absorbing powder is a composite wave-absorbing powder.
In some preferred embodiments, the composite wave-absorbing powder is selected from nano wave-absorbing materials such as graphene, carbon nano tube, ferrite and MXene-Ti, starting from wave-absorbing mechanisms such as magnetic loss and electric loss, and aiming at expanding the wave-absorbing frequency range 3 C 2 More than one of the components.
In some preferred embodiments, the composite wave-absorbing powder is made of nano wave-absorbing material graphene, carbon nanotubes, ferrite and MXene-Ti 3 C 2 Is compounded into the preparation.
In some preferred embodiments, graphene, carbon nanotubes, ferrite, and MXene-Ti 3 C 2 The mass ratio is about 4:3:2:1. In some preferred embodiments, the entrainer comprises non-polar hydrocarbon materials such as n-hexane, cyclohexane, and pentane.
In some preferred embodiments, the finishing temperature of the finishing process is 80-260 ℃, the pressure is 18-36 MPa, the finishing time is 40-100 min, and the carbon dioxide flow is 20-50 g/min.
In some preferred embodiments, the content of the wave-absorbing nano powder is 10-25% relative to the fabric to be finished.
In some preferred embodiments, the relative content of entrainer is 3 to 5%.
The after-finishing process of the supercritical carbon dioxide wave-absorbing electromagnetic shielding fabric provided by the embodiment of the invention has the advantages that no water participates in the finishing process, the operations such as cleaning and drying are not needed after finishing, the process flow is short, and the energy is saved and the environment is protected; and the unused finishing agent and the like can be recycled, so that the method has the modern processing concepts of cleanness, greenness and environmental protection.
Supercritical CO of the invention 2 No water participates in the finishing process, and the composite wave-absorbing nano powder is prepared byThe entrainer is dissolved in the supercritical carbon dioxide fluid, the finishing agent is continuously and fully contacted with the fiber interface to generate molecular acting force along with the circulating flow of the supercritical fluid, the composite wave-absorbing material is adsorbed on the surface of the fiber body along with the gradual increase of the acting force between the molecules of the composite wave-absorbing material and the molecules of the fiber, the concentration difference of the wave-absorbing material is formed between the inner part and the outer part of the fiber, and the supercritical carbon dioxide fluid has a certain swelling effect on the textile fiber, so that more composite wave-absorbing material is gradually transferred into the fiber. Meanwhile, under the super strong diffusion action of supercritical carbon dioxide fluid, the composite wave-absorbing material molecules are adsorbed with fiber macromolecules through disordered entanglement of hydrogen bonds or Van der Waals force to form a stable state.
The invention solves the technical problem that nanometer wave-absorbing materials such as ferrite, metal micropowder, graphene, carbon nano tube and the like are hard to uniformly disperse due to agglomeration in a water phase, and in a supercritical carbon dioxide dissolution system, the special lamellar structure of the graphene can be uniformly distributed among particles such as the carbon nano tube and the nano ferrite, so that the carbon nano tube and the ferrite are agglomerated again after separation and dispersion, various wave-absorbing materials can exist in a stable nano state and can be directly applied to textile materials, thereby exerting the special electrical property of the nanometer materials and exerting good electromagnetic shielding and wave-absorbing effects.
The wave-absorbing electromagnetic shielding fabric developed by the invention is mainly applied to areas with electromagnetic radiation pollution, such as factories, scientific research institutions, hospitals, railway stations, communication base stations, video monitoring command stations of public security departments and the like, in the civil field. In the military field, the electromagnetic shielding textile can be used for developing various electromagnetic shielding textiles to meet the requirements of normal operation, electromagnetic information shielding, information protection, electromagnetic stealth and the like of various electronic equipment.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following description of the embodiments will briefly describe the devices required to be used in the description of the embodiments, and it should be apparent that the following drawings are only some embodiments of the present invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flow chart of a supercritical carbon dioxide after-treatment process of a wave-absorbing electromagnetic shielding fabric provided by an embodiment of the invention.
Detailed Description
In order that those skilled in the art will better understand the present invention, a technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in which it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, shall fall within the scope of the present invention.
It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further definition or explanation thereof is necessary in the following figures.
The invention relates to a supercritical carbon dioxide after-treatment process of a wave-absorbing electromagnetic shielding fabric, which is approximately shown in figure 1 and comprises the following specific steps:
(1) And (5) fabric pretreatment. The fabric pretreatment agent is one or a mixture of more of ethanol and acetone. The treatment temperature is 40-60 ℃, the treatment time is 40-60 min, and the drying temperature is 60-80 ℃.
(2) And (5) performing supercritical carbon dioxide after-treatment. And (3) placing a certain amount of the fabric treated in the step (1) in a high-temperature high-pressure reaction kettle, and simultaneously placing a mixture of composite wave-absorbing nano powder with the mass of 10-25% and entrainer with the mass of 3-5% in a feeding kettle. Wherein the composite wave-absorbing powder comprises graphene, carbon nano tube, ferrite and MXene-Ti 3 C 2 The mass ratio of the four is controlled to be 4:3:2:1. Introducing carbon dioxide in a supercritical state after heating and pressurizing into a charging kettle at a flow of 20-50 g/min to mix and dissolve the carbon dioxide, the composite wave-absorbing nano powder and the entrainer to form a finishing agent, and under the action of a circulating device, the formed finishing agent is oxidized along with supercriticalThe carbon fluid flows back and forth between the feeding kettle and the reaction kettle. Under the condition of the temperature range of 80-260 ℃ and the pressure of 18-36 MPa, the composite wave-absorbing material dissolved in the supercritical carbon dioxide fully contacts with the fabric and then enters the fiber to realize after-treatment, the reaction temperature and the pressure are reduced after the treatment is carried out for 40-100 min, and the unused composite wave-absorbing material and gaseous CO are recycled 2 Finally, the wave-absorbing electromagnetic shielding fabric is obtained.
It should be noted that, for simplicity of description, the above-described embodiments of the method are all described as a series of combinations of actions, but it should be understood by those skilled in the art that the present invention is not limited by the order of actions described. Further, those skilled in the art will appreciate that the embodiments described in the specification are presently preferred embodiments, and that the acts are not necessarily required for the present invention.
In order to further understand the present invention, the following describes the supercritical carbon dioxide after-finishing process method of the wave-absorbing electromagnetic shielding fabric provided by the present invention in detail with reference to specific examples.
Example 1
(1) And (5) fabric pretreatment. The meta-aramid fabric is pretreated by adopting acetone. The treatment temperature is 60 ℃, the treatment time is 40min, and the drying temperature is 80 ℃.
(2) And (5) performing supercritical carbon dioxide after-treatment. Taking m 1 Placing the fabric treated in the step (1) in a high-temperature high-pressure reaction kettle, and simultaneously placing the fabric with the mass of 0.25m 1 Gram of composite wave-absorbing nano powder and 0.05m 1 The g entrainer mixture was placed in a feed kettle. Wherein the composite wave-absorbing powder comprises graphene, carbon nano tube, ferrite and MXene-Ti 3 C 2 The mass ratio of the four is 4:3:2:1. Carbon dioxide in a critical state after heating and pressurizing is introduced into a charging kettle at a flow of 20g/min, so that the carbon dioxide is mixed with the composite wave-absorbing nano powder and the entrainer to be dissolved to form a finishing agent, and the formed finishing agent flows back and forth between the charging kettle and the reaction kettle along with supercritical carbon dioxide fluid under the action of a circulating device. Under the technological conditions of 260 ℃ and 36MPa, the solution is dissolved in the supercritical fluidAfter fully contacting the composite wave-absorbing material in the carbon oxide with the fabric, entering the inside of the fiber to realize after-treatment, reducing the reaction temperature and the reaction pressure after 100min of treatment, and recycling the unused composite wave-absorbing material and gaseous CO 2 Finally, the wave-absorbing electromagnetic shielding fabric is obtained.
Example two
And (5) fabric pretreatment. And (3) preprocessing the meta-aramid fiber and flame-retardant viscose blended fabric by adopting ethanol. The treatment temperature is 40 ℃, the treatment time is 60min, and the drying temperature is 60 ℃.
And (5) performing supercritical carbon dioxide after-treatment. Taking m 2 Placing the fabric treated in the step (1) in a high-temperature high-pressure reaction kettle, and simultaneously placing the fabric with the mass of 0.15m 2 Gram of composite wave-absorbing nano powder and 0.03m 2 The g entrainer mixture was placed in a feed kettle. Wherein the composite wave-absorbing powder comprises graphene, carbon nano tube, ferrite and MXene-Ti 3 C 2 The mass ratio of the four is 4:3:2:1. Carbon dioxide in a critical state after heating and pressurizing is introduced into a charging kettle at a flow rate of 30g/min, so that the carbon dioxide is mixed with the composite wave-absorbing nano powder and the entrainer to be dissolved to form a finishing agent, and the formed finishing agent flows back and forth between the charging kettle and the reaction kettle along with supercritical carbon dioxide fluid under the action of a circulating device. Under the process conditions of 220 ℃ and 32MPa, the composite wave-absorbing material dissolved in the supercritical carbon dioxide fully contacts with the fabric and enters the fiber to realize after-treatment, the reaction temperature and the reaction pressure are reduced after the treatment is carried out for 60min, and the unused composite wave-absorbing material and gaseous CO are recovered 2 Finally, the wave-absorbing electromagnetic shielding fabric is obtained.
Example III
And (5) fabric pretreatment. And preprocessing the flame-retardant polyester and flame-retardant viscose blended fabric by adopting ethanol. The treatment temperature is 50 ℃, the treatment time is 50min, and the drying temperature is 60 ℃.
And (5) performing supercritical carbon dioxide after-treatment. Taking m 3 Placing the fabric treated in the step (1) in a high-temperature high-pressure reaction kettle, and simultaneously placing the fabric with the mass of 0.1m 3 Gram of composite wave-absorbing nano powder and 0.03m 3 The g entrainer mixture was placed in a feed kettle. Wherein the method comprises the steps ofThe composite wave-absorbing powder comprises graphene, carbon nano tube, ferrite and MXene-Ti 3 C 2 The mass ratio of the four is 4:3:2:1. Carbon dioxide in a critical state after heating and pressurizing is introduced into a charging kettle at a flow rate of 30g/min, so that the carbon dioxide is mixed with the composite wave-absorbing nano powder and the entrainer to be dissolved to form a finishing agent, and the formed finishing agent flows back and forth between the charging kettle and the reaction kettle along with supercritical carbon dioxide fluid under the action of a circulating device. Under the process conditions of 80 ℃ and 20MPa, the composite wave-absorbing material dissolved in the supercritical carbon dioxide fully contacts with the fabric and enters the fiber to realize after-treatment, the reaction temperature and the reaction pressure are reduced after the treatment is carried out for 60min, and the unused composite wave-absorbing material and gaseous CO are recovered 2 Finally, the wave-absorbing electromagnetic shielding fabric is obtained.
Electromagnetic shielding performance test
In order to verify the performance of the prepared fabric, the 3-pattern wave-absorbing electromagnetic shielding fabric prepared in examples 1-3 is subjected to shielding performance according to GJB 6190-2008 "method for testing shielding effectiveness of electromagnetic shielding Material", and wave-absorbing performance (emissivity) is performed according to GJB 2038A-2011 "method for testing reflectivity of radar wave-absorbing Material".
Meanwhile, in order to verify the electromagnetic shielding performance of the sample after the supercritical carbon dioxide after-treatment process of the wave-absorbing electromagnetic shielding fabric, performance comparison test is carried out with the commercial wave-absorbing electromagnetic shielding fabric on the market. An electromagnetic shielding fabric (silver loaded) of a manufacturer in Qingdao, shandong was used as a sample of comparative example one.
In addition, the positive influence of the supercritical carbon dioxide after-finishing process of the wave-absorbing electromagnetic shielding fabric on the shielding performance of the fabric is highlighted for longitudinal comparison. The pretreated fabric of example 1 was used without treatment by supercritical carbon dioxide finishing process, and the sample obtained by conventional finishing process was comparative example two. In the compared samples, meta-aramid, flame-retardant viscose and flame-retardant polyester all have no wave-absorbing function, so that the influence on the electromagnetic shielding and wave-absorbing performance of the samples is ignored in comparison analysis. Five fabrics were cut out for five different areas of the samples of examples one to three and two comparative examples as test samples, respectively, with the test bands set at 4GHz to 14GHz, and the test results are shown in table 1.
Table 1 electromagnetic shielding and emissivity test results for each sample
The above test results show that in the 4 GHz-14 GHz band, the average value of the electromagnetic shielding performance of the first embodiment is 53.0dB, the average value of the electromagnetic shielding performance of the second embodiment is 48.0dB, and the average value of the electromagnetic shielding performance of the third embodiment is 42.9dB. Compared with the shielding performance of the first and second comparative examples, the electromagnetic shielding performance of the wave-absorbing electromagnetic shielding fabric treated by the supercritical carbon dioxide after-treatment process is improved by more than 30%. In terms of wave-absorbing performance, the average value of the reflectivity of the first embodiment is-26.9 dB, the average value of the reflectivity of the first comparative embodiment is-2.5 dB, and compared with the traditional electromagnetic shielding fabric, the wave-absorbing electromagnetic shielding fabric developed by the invention is excellent in wave-absorbing performance, the average value of the reflectivity of the second comparative embodiment is-11.6 dB, and the content and uniformity of wave-absorbing composite powder in fabric distribution can be improved by using a supercritical carbon dioxide after-finishing process, so that the prepared wave-absorbing electromagnetic shielding fabric is excellent in wave-absorbing performance. Meanwhile, the test results show that the shielding performance and the data dispersion coefficient of the wave absorbing performance of different areas are small, and the carbon dioxide supercritical after-treatment process of the invention also shows that the dispersibility of the wave absorbing powder in a system is improved.
In the foregoing embodiments of the present invention, the descriptions of the embodiments are emphasized, and for a portion of this disclosure that is not described in detail in this embodiment, reference is made to the related descriptions of other embodiments.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (3)
1. A supercritical carbon dioxide after-finishing method of a wave-absorbing electromagnetic shielding fabric comprises the following specific steps:
(1) Pretreating the fabric, and drying the fabric for later use;
the fabric pretreatment agent is one or a mixture of more of ethanol and acetone;
the pretreatment temperature is 40-60 ℃, the treatment time is 40-60 min, and the drying temperature is 60-80 ℃;
(2) Post-treatment of supercritical carbon dioxide: taking a certain amount of pretreated fabric, placing the fabric in a high-temperature high-pressure reaction kettle, and simultaneously placing a mixture of composite wave-absorbing nano powder and entrainer in a feeding kettle; the composite wave-absorbing nano powder comprises nano wave-absorbing material graphene, carbon nano tube, ferrite and MXene-Ti 3 C 2 Wherein the nano wave-absorbing material comprises graphene, carbon nano tube, ferrite and MXene-Ti3C 2 The mass ratio is 4:3:2:1; the entrainer is selected from n-hexane, cyclohexane or pentane;
introducing carbon dioxide fluid which is in a supercritical state after heating and pressurizing into a charging kettle, and mixing and dissolving the carbon dioxide fluid, the composite wave-absorbing nano powder and the entrainer to form a finishing agent; the composite wave-absorbing nano powder is dissolved in supercritical carbon dioxide fluid under the action of entrainer;
under the action of a circulating device, the finishing agent flows back and forth between the feeding kettle and the reaction kettle along with the supercritical carbon dioxide fluid, molecular acting force is generated when the finishing agent contacts with a fiber interface, the composite wave-absorbing material is adsorbed on the surface of the fiber body, the concentration difference of the wave-absorbing material is formed inside and outside the fiber, and meanwhile, more composite wave-absorbing material is transferred into the fiber through the swelling action of the supercritical carbon dioxide fluid on the textile fiber;
under the super strong diffusion action of supercritical carbon dioxide fluid, the composite wave-absorbing nano powder molecules are adsorbed with fiber macromolecules through disordered entanglement of hydrogen bonds or Van der Waals forces to form a stable state;
(3) Post-treatment: after 40-100 min, reducing the reaction temperature and pressure to separate the unused composite wave-absorbing powder from the carbon dioxide in a separation kettle, and recycling the unused composite wave-absorbing material and the gaseous carbon dioxide;
the after-finishing process is free of water participation, and cleaning and drying operations are not needed after finishing.
2. The supercritical carbon dioxide after-finishing method for the wave-absorbing electromagnetic shielding fabric according to claim 1, wherein the after-finishing process is carried out at a finishing temperature of 80-260 ℃, a pressure of 18-36 MPa, a finishing time of 40-100 min and a carbon dioxide flow of 20-50 g/min.
3. The supercritical carbon dioxide after-treatment method of the wave-absorbing electromagnetic shielding fabric, according to claim 1, wherein the content of the composite wave-absorbing nano powder is 10-25% relative to the fabric to be treated, and the content of the entrainer is 3-5% relative to the fabric to be treated.
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